Laboratory apparatus for the chemical modification of packaged yarns



NOV. 4, 1969 D, STANQNIS ETAL Y 3,475,823.

LABORATORY APPARATUS FOR THE CHEMICAL MODIFICATION OF PACKAGED YARNS 3 Sheets-Sheet 1 Filed Dec. 23, 1965 FIGZ INVENTORS DAVID J. STANONIS WALTER 0 KING CHARLES R- ESPOSITO ATTORN D. J. STANONIS ETAI- 3,475,323 LABORATORY APPARATUS FOR THE CHEMICAL Nov. 4, 1969 3 Sheets-Sheet 2 Filed Dec. 23. 1965 0 0 0 00 0 0 000 00000 0 0 000 000w; o o qo o o o o o 0 o 0 0 o o 0 o o O O O O O O O O O O G O O 0 0 0 0 0006 OOOOO 0006 woooooooooooooo o o o ooooooooo oo 0 INVENTORS DAVID J. STANONlS WALTER D. KING CHARLES RESPOSITO FIG.4

ATTORNEY NOV. 4, 1969 J s No s'ETAL 3,475,823

LABORATORY APPARATUS FOR THE CHEMICAL MODIFICATION OF PACKAGED YARNS 3 Sheets-Sheet 3 Filed Dec. 23, 1965 QUE 5 t2: 58308915 5.". 950% 663$ md 0 o; v; N4 04 w o v N. 00 m M e N 3 M e w 5 .1 v D 3 w IL 9 m l M D H I m; Q l S o I w. L m;

DAVID J.STANON|S WALTER D. KING CHARLES RESPOSITO United States Patent 3,475,823 LABORATORY APPARATUS FOR THE CHEMICAL MODIFICATION OF PACKAGED YARNS David J. Stanonis and Walter D. King, New Orleans, and

Charles R. Esposito, Chalmette, La., assignors to the United States of America as represented by the Secretary of Agriculture Filed Dec. 23, 1965, Ser. No. 516,026 Int. Cl. G01b 5/00 US. Cl. 33-125 1 Claim A non-exclusive, irrevocable, royalty-free license in the invention herein described, throughout the world for all purposes of the United States Government, with the power to grant sublicenses for such purposes, is hereby granted to the Government of the United States of America.

This invention relates to an apparatus for the chemical modification of packaged yarns. More specifically, this invention relates to an apparatus for the chemical modification of packaged yarns which voids the tensioning undergone by the yarns in the process of the chemical modification.

The main objective of this invention is to provide an apparatus which will yield to the excess tension caused by some chemical modifications of yarns in package form.

Another objective of this invention is to provide an apparatus for the chemical modification of packaged yarns which will not only withstand the tensioning of the yarns caused by the chemical modification but also will withstand the corrosive action of the chemicals.

Available apparatus being used presently for package dyeing and chemical modification is made of stainless steel. Such equipment does not allow for chemical treatments which both damage the stainless steel and submit the yarn being treated in the package form to high tension, tension at times breaks the yarn and at other times corrosion damages the equipment. One of the more common chemical treatments performed on package machines is the mercerization of cellulosic yarns. This particular treatment swells the fibrils thereby shortening the yarn. The strength imparted to the fibrils by this treatment is such that the available stainless steel tubes may be crushed by the tension or the yarn submitted to the treatment may be unevenly mercerized under tension. Mercerization per se adds strength to the yarns of cotton; however, other chemical treatments do not add strength and cause breakage under the tension of the treatment. It is for this reason that We have felt it necessary to invent an apparatus which would both withstand the chemical corrosion of the treatment and allow for the tension to which the packaged yarns are subjected as they change in physical and chemical characteristics.

We have discovered that all the surfaces touched by the chemical substances involved in the treatment of the textile yarns need not be corroded. By process of our invention corrosive chemical reactions can be carried out without damage to the yarn being processed and without damage to the surfaces of the equipment being utilized for the chemical modification. All the surfaces touched by the treating chemical can be coated with Teflon, and the assembly can be made up of various nonreacting materials.

The perforated Teflon sheet is made somewhat similar to the standard perforated cylinder; however, it differs in that the Teflon sheet is free to diminish in size as needed for yarn contraction by progressive involution of the 3,475,823 Patented Nov. 4, 1969 coiled sheet. There are other specific details about the design of this perforated cylinder, which are more precisely explained below.

The apparatus which is our invention can best be described as a device made entirely of chemically resistant materials, and designed specifically for the chemical reactions of cotton and other cellulosic and noncellulosic yarns with organic reagents at elevated temperatures.

The need for this apparatus was felt mostly strongly in the laboratory where a systematic study of the effects of different substituents introduced heterogeneously into the cellulose molecule, for instance, upon the physical and textile properties of the yarns would be carried out. The proper evaluation of the finished yarns could not be accomplished accurately, since the yarns would be treated at various tensions during the interim of the reaction. It has been felt that quantities of one-tenth of a pound or more of treated yarns cannot be prepared for investigation of the properties imparted to the yarns being processed because the reaction between yarns and reactants has not been carried out at any particular tension, that is, the tension has changed as the reaction proceeds, and the different regions of the packaged yarn have been submitted to a nonuniform treatment.

Apparatus available for the laboratory treatment and chemical modification of cellulosic and other yarns were found to be definitely not suitable. In particular the package dyeing machine which is commonly used in the textile industry was judged inadequate in that the stainless steel cannot withstand the reaction media of modern research, among which are trifiuoroacetic anhydride, alkyl and acyl halides, sulfuric and other acids, zinc fluoborate and the like which are generally employed as catalysts, and a long innumerable list of chemical reagents and solvents used in the textile industries. A laboratory device described by Albert S. Cooper, Jr., et al., in Textile Industry, vol. 116, No. 1 (1952), where the partial acetylation of cotton fibers, yarns, and fabrics is carried out, and which later was modified by Edmund M. Buras et al. in Textile Research Journal, vol. 27 (1957) was judged inadequate in both instances in that no means are provided for the control of tension of the yarn while permitting contraction, and again the metal of the pump and the rubber hose connections cannot be considered adequate for these cannot resist the corrosiveness of the reagents nor the temperatures utilized in the modern laboratory. The laboratory apparatus used by Norton Cashen et al., Textile Research Jour., vol. 27 (1957) employs metals for heat transfer. This apparatus also is considered unsuitable because the metals employed cannot withstand some of the reagents of modern research.

In view of the failures of the available equipment and processes we found it necessary to design our own apparatus, and piece by piece after some failures and modifications in the process of our investigations with cotton, were able to invent and assemble the device which could perform all the tasks that were required of it for the treatment of textile yarns.

The problem was solved by wrapping the test yarn onto a tube, the body of which consists of a coiled perforated sheet, resting on facing cone ends. The initial, relatively large diameter of the tube is then free to diminish as needed for yarn contraction by progressive involution of the coiled sheet and corresponding separation of the cone ends. By a spring mechanism the tension, required to reduce or enlarge the diameter of the tube for contraction or extension of the yarn, can be regulated. We have invented and reported this apparatus in Textile Research Journal, vol. 35, No. 1, January 1965, in an article entitled A New Laboratory Apparatus for Use in Chemical Modification of Packaged Cellulosic Yarns. In spite of the limited use implied by the title, we have since discovered that many and varied modifications can be made to the apparatus in order to process larger quantities, as well as to make the device adaptable to the available larger package processing machines.

In order to illustrate the invention we submit the several figures below, which are specifically of the apparatus for the processing of a fraction of a pound or more, and should not be construed as limiting the scope of the invention. The figures shown are as follows:

FIGURES 1 and 2 show two views of the yarn holder assembly, specifically a perspective view and a cut-away auxiliary elevation view, both correlated views illustrate the apparatus while center shaft is in the vertical position.

FIGURE 3 is a top view of the perforated Teflon sheet 1 showing the beveled edges and 11.

FIGURE 4 is a front view of the perforated Teflon sheet 1. The perforated Teflon sheet 1 is a trapezoid. The edges 10 and 11 are parallel to each other. The edges 12 and 13 are tapered about 2 /2".

Referring to FIGS. 1 to 4 inclusive. Referring to FIG. 1 drawing of the essential parts of the special yarn holder: It is comprised of the following parts: a coiled perforated Teflon sheet, trapezoidal in shape, 1 showing the beveled edges 10 and 11 which are parallel to each other. The edges 12 and 13 are tapered about 2 /2".

The concentric, hollow nylon tube 2 is perforated between cone ends with external threads on each end. The lower end is threaded internally and plugged with a nylon screw. The upper Teflon cone 3 with shoulder is bored to a sliding fit to the nylon tube 2.

The lower Teflon cone 4 with shoulder and with internal threads is screwed onto the lower end of the nylon tube 2.

The hollow glass tube 9 is a spacer which rests upon the upper Teflon cone 3. The lower Teflon bushing 8 with shoulder is bored to a sliding fit to the nylon tube 2. The bushing 8 is used to center the tensioning spring which rests atop the glass spacer 9, and receives the lower end of the Teflon coated tensioning spring 5. The upper Teflon bushing 7 with shoulder which is also used to center the tensioning spring is bored to a sliding fit to the nylon tube 2. It receives the upper end of the tensioning spring. The tensioning nut 6 is used to regulate the tension.

In operation the coiled Teflon sheet 1 is held in place, away from the concentric tube 2, by mounting it between facing cone ends 3 and 4. The upper cone 3 is free to slide on the inner tube 2, while the lower is screwed onto the bottom of the tube 2. The bottom end of tube 2 is plugged. Tension is regulated by parts 5, 6, 7, 8, and 9.

As reaction takes place or as the yarn reacts the coiled Teflon sheet 1 forces itself away from fixed cone 4, and forces movable cone 3 away from coiled sheet. The degree of movement of cone 3 and coiled sheet 1 is governed by the Teflon coated tension spring 5, Teflon tension nut 6, Teflon tension spring centering bushings of 7 and 8, and glass spacer tube 9.

The coiled Teflon sheet 1 is feathered on the leading and trailing edges and is tapered on the top and bottom edges that are in contact with cones 3 and 4.

The purpose of the taper is to make a better seal with the cones so little liquid pressure is lost.

7 ID. holes are spaced in the greater portion of the Teflon sheet 1, and ,5 ID. holes are spaced near the top and bottom edges or near the contact area with the cones 3 and 4.

The upward displacement of the movable cone 3 is a function of the extent of reaction the yarn has undergone. More specifically, the swelling of the yarn causes a reduction of the inner diameter of the packaged yarn. This, in turn, causes the ejection of the cone 3 away from the center of the assembly. The ejection of the cones causes the displacement of the centering bushing. This displacement, when the axis of the assembly is vertical, can be called an upward displacement. The displacement of this centering bushing can be measured, and the upper limit of the displacement is related to the sum total of the height of the cones. This upper limit can be changed if the dimensions of the assembly are changed either to suit the use of a larger assembly or a smaller assembly.

The relationship between bushing displacement and extent of reaction the yarn has undergone can readily be computed. There is a linear relationship in most reactions wherein a definite amount of upward displacement of the centering bushing is proportional to the degree of substitution of the treated yarn, and generally the degree of substitution arrived at during a reaction can readily be seen while the reaction is still in progress. A calibration curve can be prepared by running a series of yarn package reactions, each of which produces a different upward displacement. This would yield a set of yarns which when analyzed for degree of substitution would have five different D.S. values. From these data the correlation can be made, and the calibration curve established.

FIGURE 5 illustrated such a calibration curve, which was prepared from a planned series of experiments. For this particular curve five approximately one-tenth pound package reactions were reacted separately, to give five different displacements. For this series an aliphatic acid chloride was reacted with the selected cotton yarn, and the reaction was carried out in the presence of pyridine. The displacement of the centering bushing for each package was recorded, and the yarn was submitted to elemental analysis. The results of the analysis were converted to 13.8., and the correlation was obtained as desired for the preparation of this calibration curve of FIGURE 5.

It was decided from this and other similar investigations that extent of reaction could be very accurately predicted by stopping the reaction at the point indicated by the established calibration curve. For this particular series, using an assembly which could be adaptable to available package dyeing machines, we were able to observe displacement about from 0.1 to 1.7 inches for a correlated D5. of about from 0.1 to 1.7 alkyl groups per anhydroglucose unit. This particular linearity is not necessarily applicable to all the known reactions, since some substances will react with cotton without noticeable swelling of the cotton. However, the equipment can be fabricated to meet the needs of the particular degree of swelling. A great amount of swelling can be toned down by fabricating cones which will have a larger diameter, while a low amount of swelling can be made more pronounced by employing cones with a smaller diameter. Such cones would be made of the same material but would require less constriction from the yarn to be expelled, when the diameter of the cone would be small, and more constriction from the yarn when the diameter of the cone would be larger. Again, of course there may be some reactions that would possibly cause no swelling of the yarns. For this particular reaction the invention is not utilizable.

We claim:

1. A generally rectilinear foraminous sheet coiled resiliently to describe at least one complete convolution; a mandrel spaced centrally within the coiled foraminous sheet; a first conic member with apex directed inwardly, located at one end of, concentric, and stationary relative said mandrel; a second conic member with apex directed inwardly, concentric, and movable axially on said mandrel; said second conic member spaced from said first conic member approximately the coiled width of said sheet; resilient means adjustable with respect to resilient load, linking said second conic member and said mandrel, said resilient means adapted to resist axial movement of said second conic member away from said first conic member; the curved surfaces of said conic members adapted to support the lateral coiled edges of said sheet; whereby compression coiling of said sheet acts to separate the conic members axially and slack uncoiling of said sheet acts to converge the conic members axially; and graduated scale indicia means on said mandrel adapted to permit measurement of the relative axial movement of the conic members.

References Cited FOREIGN PATENTS 651,400 3/1951 Great Britain.

5 LEON D. ROSDOL, Primary Examiner I. D. \WELSH, Assistant Examiner US. Cl. X.R. 

1. A GENERALLY RECTILINEAR FORAMINOUS SHEET COILED RESILIENTLY TO DESCRIBE AT LEAST ONE COMPLETE CONVOLUTION; A MANDREL SPACED CENTRALLY WITHIN THE COILED FORAMINOUS SHEET; A FIRST CONIC MEMBER WITH APEX DIRECTED INWARDLY, LOCATED AT ONE END OF, CONCENTRIC, AND STATIONARY RELATIVE SAID MANDREL; A SECOND CONIC MEMBER WITH APEX DIRECTED INWARDLY, CONCENTRIC, AND MOVABLE AXIALLY ON SAID MANDREL; SAID SECOND CONIC MEMBER SPACED FROM SAID FIRST CONIC MEMBER APPROXIMATELY THE COILED WIDTH OF SAID SHEET; RESILIENT MEANS ADJUSTABLE WITH RESPECT TO RESILIENT LOAD, LINKING SAID SECOND CONIC MEMBER AND SAID MAN- 